US5738733A - Ferrous metal glassy alloy - Google Patents

Ferrous metal glassy alloy Download PDF

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Publication number
US5738733A
US5738733A US08657786 US65778696A US5738733A US 5738733 A US5738733 A US 5738733A US 08657786 US08657786 US 08657786 US 65778696 A US65778696 A US 65778696A US 5738733 A US5738733 A US 5738733A
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alloy
metal
glassy
temperature
invention
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US08657786
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Akihisa Inoue
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BMG Co Ltd
Research Development Corp of Japan
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Research Development Corp of Japan
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/02Amorphous alloys with iron as the major constituent
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni

Abstract

The present invention provides a ferrous metal glassy alloy having temperature interval ΔTx of supercooled liquid as expressed by the following formula:
ΔTx=Tx-Tg
(where, Tx is an onset temperature of crystallization, and Tg is a glass transition temperature) of at least 40 K, which realizes magnetic properties as a bulky alloy.

Description

BACKGROUND OF THE INVENTION

1. Field of the Invention

The present invention relates to a ferrous metal glassy alloy. More particularly, the present invention relates to a novel metal glassy alloy, available as a bulky alloy having a far larger thickness than a conventional amorphous alloy thin ribbon, excellent in magnetic properties.

2. Description of Related Art

Some of the conventional multi-element alloys are known to have a wide temperature region in which they are in a state of a supercooled liquid before crystallization and constitute metal glassy alloys. It is also known that these metal glassy alloys form bulky alloys having a far larger thickness than the conventionally known amorphous alloy thin ribbon.

The metal glassy alloys known as above include Ln-Al-TM, Mg-Ln-TM, Zr-Al-TM, Hf-Al-TM, and Ti-Zr-Be-TM (where, Ln is a lanthaned metal and TM indicates a transition metal).

However, none of these conventionally known metal glassy alloys are magnetic at room temperature, and this has lead to a significant restriction in industrial uses.

These alloys, while showing the supercooled liquid state, have no practicability because of a small temperature interval ΔTx of the supercooled liquid region, i.e., the difference (Tx-Tg) between the onset temperature of crystallization (Tx) and the glass transition temperature (Tg), practically resulting in a poor metal glass-forming ability. To judge from this fact, the presence of an alloy which has a wide temperature region of supercooled liquid and is capable of forming a metal glass through cooling would overcome the thickness restriction imposed on a conventional amorphous alloy thin ribbon and should metallurgically attract the general attention. In practice, however, the conventional metal glassy alloys which are not magnetic at room temperature have been under inevitable limitations.

SUMMARY OF THE INVENTION

The present invention was developed in view of the above-mentioned circumstances, and has an object to provide a novel metal glassy alloy which overcomes the limits in the conventional technology, permits manufacture as a bulky metal, and further allows application as a magnetic material.

The present invention provides a ferrous metal glassy alloy which comprises a ferrous alloy having a temperature interval ΔTx of a supercooled liquid as expressed by the following formula:

ΔTx=Tx-Tg

(where, Tx is an onset temperature of crystallization, and Tg is a glass transition temperature) of at least 40 K.

The present invention provides also embodiments wherein the above-mentioned alloy contains, together with iron, other metal and semi-metal elements, wherein the other metal elements are at least one selected from the group consisting of the metal elements of the III-B group and the IV-B group, and wherein the semi-metal elements are at least one selected from the group consisting of phosphorus, carbon, boron, silicon and germanium.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 shows a photograph of an electron diffraction pattern in place of a drawing of Example 1;

FIG. 2 shows an X-ray diffraction pattern of Example 1;

FIG. 3 shows a DSC curve of Example 1;

FIG. 4 shows a B-H curve of Example 1;

FIG. 5 shows an X-ray diffraction of Example 2;

FIG. 6 shows a DSC curve of Example 2; and

FIG. 7 shows a B-H hysteresis curve of Example 2.

DETAILED DESCRIPTION OF THE INVENTION

As described above, the present invention provides a novel magnetic metal glassy alloy at room temperature, which permits formation of a bulky alloy so far unknown.

Among ferrous alloys, Fe-P-C, Fe-P-B and Fe-Ni-Si-B ones are observed to exhibit glass transition. These alloys have however a very small temperature interval ΔTx of up to 25 K of the supercooled liquid, and cannot practically form metal glassy alloys. The metal glassy alloy of the present invention has in contrast a temperature interval ΔTx of the supercooled liquid of at least 40 K or even at least 60 K, which represents a remarkable temperature region which has not been anticipated at all to date as a ferrous alloy from conventional findings. Furthermore, the alloy of the present invention excellent also in magnetic properties is actually novel and is far superior in practical applicability to the conventional amorphous alloys applicable only as thin ribbons.

The alloy of the present invention is characterized by a chemical composition, as described above, mainly comprising iron and containing other metal and semi-metal elements. Of these, the other metal elements may be selected from the group consisting of metal elements of the II-A group, the III-A and III-B groups, the IV-A and IV-B groups, the V-A group, the VI-A group and the VII-A group, or more appropriately, metal elements of the III-B group and the IV-B group, including, for example, aluminum, gallium, indium and tin.

Such metals as titanium, hafnium, copper, manganese, niobium, molybdenum, chromium, nickel, cobalt, tantalum and tungsten may also be blended.

Applicable semi-metal elements include, for example, phosphorus, carbon, boron, silicon and germanium.

More specifically, the ferrous metal glassy alloy of the present invention comprises, in the following amounts, in atomic percentage:

______________________________________aluminum           from 1 to 10%,gallium            from 0.5 to 4%,phosphorus         from 9 to 15%,carbon             from 5 to 7%,boron              from 2 to 10%, andiron               balance______________________________________

and may contain incidental impurities. Also it may contain from 0.5 to 2% silicon or 0.5 to 4% germanium.

Another embodiment covers an alloy composition containing, in addition to any of niobium, molybdenum, chromium, hafnium, tantalum and tungsten in an amount of up to 7%, up to 10% nickel and up to 30% cobalt.

In any of the embodiments of the present invention, the ferrous metal glassy alloy has a temperature interval ΔTx of a supercooled liquid of at least 40 K, or even at least 60 K.

In the present invention as described above, the metal glassy alloy can be manufactured through melting and casting, or quenching by means of a single roll or dual rolls, or further the in-rotating-liquid spinning process or the solution extraction process, or the high-pressure gas atomization, into bulk, ribbon, wire or powder shape. In this manufacture, there is available an alloy having a thickness and a diameter more than ten times as large as those for the conventional amorphous alloy.

These alloys show magnetism at room temperature and a better magnetism as a result of an annealing treatment. They are therefore useful for various applications as a material having excellent soft ferromagnetic properties.

As to manufacture, it should be added that an optimum cooling rate, depending upon the chemical composition of the alloy, means for manufacture, and size and shape of the product, may usually be set within a range of from 1 to 102 K/s as a standard. In practice, the cooling rate may be determined by confirming whether or not such crystal phases as Fe3 B, Fe2 B, or Fe3 P precipitates in the glassy phase.

Now, the metal glassy alloy of the present invention is described further in detail by means of working examples.

EXAMPLE 1

Iron, aluminum and gallium metals, an Fe-C alloy, an Fe-P alloy and boron as raw materials were induction-melted in an argon atmosphere, and cast into an alloy ingot of Fe72 Al5 Ga2 P11 C6 B4 in atomic ratio. A ribbon having a cross-sectional area of 0.02×1.5 mm2 was prepared in an argon atmosphere from the thus prepared ingot by the single roller melt-spinning process. It was confirmed through an X-ray diffraction and a TEM that the resultant ribbon had a metal glassy nature. Glass transition and crystallization were evaluated by means of a differential scanning calorimeter (DSC).

FIGS. 1 and 2 illustrate an electron diffraction pattern and an X-ray diffraction pattern, both demonstrating that the above alloy is of the glassy phase. FIG. 3 illustrates a DSC curve, suggesting that the alloy has a temperature interval of supercooled liquid, which represents the temperature difference (Tx-Tg) between the glass transition (Tg) temperature and the onset temperature of crystallization (Tx) of 61 K.

As a result of measurement at a scanning rate of 0.33 K/s by means of a differential thermal analyzer (DTA), the above alloy has a melting point (Tm) of 1,271 K, giving a ratio Tg/Tm of 0.58.

Evaluation of magnetic properties of the alloy revealed that the as-quenched alloy and the alloy after an annealing treatment at 723 K for 600 s exhibited hysteresis B-H curves with 1.59 kA/m at room temperature as shown in FIG. 4, respectively. Bs, He, λs and μe were as shown in Table 1.

              TABLE 1______________________________________        As-quenched                Annealed______________________________________Bs (T)          1.07     1.07Hc (A/m)       12.7      5.1λs      2.0 × 10.sup.-6                    --μc          3600      9000at 1 kHz______________________________________

This result suggests that the above-mentioned metal glassy alloy has excellent soft ferromagnetic properties.

EXAMPLE 2

An alloy having an atomic composition of Fe73 Al5 Ga2 P11 C5 B4 was melted in the same manner as in Example 1, and a bar-shaped alloy sample having a circular cross-section was prepared through injection molding in a copper die. The sample had a length of about 50 mm and a diameter of from 0.5 to 2.0 mm. Forming was carried out under a pressure of 0.05 MPa.

Observation of the outer surface permitted confirmation that the alloy has a smooth surface and a satisfactory metallic gloss, with a good formability. Then, after etching the alloy with a solution comprising 0.5% hydrofluoric acid and 99.5% distilled water at 293 K for 10 s, the cross-section was observed by means of an optical microscope. This microscope observation revealed that a crystal phase was non-existent and the alloy comprised a glassy phase.

The results of an X-ray diffraction analysis for samples having a diameter of 0.5 mm and 1.0 mm are shown in FIG. 5: broad peaks are observed only at and around a 2θ of 43.6° and a peak corresponding to a crystal phase is not found at all. This suggests the fact that, even with a diameter of 1.0 mm, the resultant alloy comprises a glassy phase.

FIG. 6 illustrates DSC curves for alloy samples having diameters of 0.5 mm and 1.0 mm and a ribbon sample as in Example 1. In all cases, the curves demonstrate a glass transition temperature (Tg) of 732 K, an onset temperature of crystallization (Tx) of 785 K and a temperature interval of supercooled liquid (ΔTx) of 53 K.

FIG. 7 shows a hysteresis B-H curve. Magnetic properties were confirmed to be equivalent with those in Example 1.

It is needless to mention that the present invention is not limited at all by the above-mentioned examples, and that various embodiments are possible as to its chemical composition, manufacturing process, annealing treatment, shape and the like.

According to the present invention, as described above in detail, there is provided a ferrous metal glassy alloy which overcomes the restrictions such as the thickness of conventional amorphous alloy thin ribbon, can be supplied as a bulky alloy, and is expected to be applicable as a material having magnetic properties.

Claims (8)

What is claimed is:
1. A ferrous metal glassy alloy, comprising at least one metal selected from the group consisting of aluminum, gallium, indium and tin, at least one semi-metal element selected from the group consisting of phosphorus, carbon, boron, silicon, and germanium, with the balance being iron, and
wherein the ferrous metal glassy alloy has a temperature interval ΔTx of a supercooled liquid of at least 40 K, as determined by the following formula:
ΔTx=Tx-Tg
where Tx is an onset temperature of crystallization and Tg is a glass transition temperature.
2. The ferrous metal glassy alloy according to claim 1, comprising, in atomic percentage:
from 1 to 10% aluminum,
from 0.5 to 4% gallium,
from 9 to 15% phosphorus,
from 5 to 7% carbon,
from 2 to 10% boron, and
the balance being iron,
wherein the alloy may contain incidental impurities.
3. The ferrous metal glassy alloy according to claim 2, further comprising from 0.5 to 2% silicon.
4. The ferrous metal glassy alloy according to claim 2, further comprising 0.5 to 4% germanium.
5. The ferrous metal glassy alloy according to claim 1, further comprising up to 7%, in atomic percentage, of at least one element selected from the group consisting of niobium, molybdenum, hafnium, tantalum, tungsten and chromium.
6. The ferrous metal glassy alloy according to claim 1, further comprising up to 10%, in atomic percentage, of nickel.
7. The ferrous metal glassy alloy according to claim 1, further comprising up to 30%, in atomic percentage, of cobalt.
8. The ferrous metal glassy alloy according to claim 1, which is annealed.
US08657786 1995-06-02 1996-05-31 Ferrous metal glassy alloy Expired - Lifetime US5738733A (en)

Priority Applications (2)

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JP13679295A JP3904250B2 (en) 1995-06-02 1995-06-02 Fe-based metallic glass alloy
JP7-136792 1995-06-29

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US5961745A (en) * 1996-03-25 1999-10-05 Alps Electric Co., Ltd. Fe Based soft magnetic glassy alloy
US5976274A (en) * 1997-01-23 1999-11-02 Akihisa Inoue Soft magnetic amorphous alloy and high hardness amorphous alloy and high hardness tool using the same
US6077367A (en) * 1997-02-19 2000-06-20 Alps Electric Co., Ltd. Method of production glassy alloy
US6086651A (en) * 1997-08-28 2000-07-11 Alp Electric Co., Ltd. Sinter and casting comprising Fe-based high-hardness glassy alloy
US6183889B1 (en) * 1997-08-28 2001-02-06 Alps Electric Co., Ltd. Magneto-impedance element, and magnetic head, thin film magnetic head, azimuth sensor and autocanceler using the same
US6331348B1 (en) 1997-10-20 2001-12-18 Alps Electric Co., Ltd. Substrate having repaired metallic pattern and method and device for repairing metallic pattern on substrate
US6350323B1 (en) 1999-01-08 2002-02-26 Alps Electronic Co., Ltd. High permeability metal glassy alloy for high frequencies
US6594157B2 (en) 2000-03-21 2003-07-15 Alps Electric Co., Ltd. Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US20030164209A1 (en) * 2002-02-11 2003-09-04 Poon S. Joseph Bulk-solidifying high manganese non-ferromagnetic amorphous steel alloys and related method of using and making the same
US20050236071A1 (en) * 2004-04-22 2005-10-27 Hisato Koshiba Amorphous soft magnetic alloy powder, and dust core and wave absorber using the same
US20050263216A1 (en) * 2004-05-28 2005-12-01 National Tsing Hua University Ternary and multi-nary iron-based bulk glassy alloys and nanocrystalline alloys
US20060130944A1 (en) * 2003-06-02 2006-06-22 Poon S J Non-ferromagnetic amorphous steel alloys containing large-atom metals
US20060213587A1 (en) * 2003-06-02 2006-09-28 Shiflet Gary J Non-ferromagnetic amorphous steel alloys containing large-atom metals
US20070258842A1 (en) * 2005-11-16 2007-11-08 Zhichao Lu Fe-based amorphous magnetic powder, magnetic powder core with excellent high frequency properties and method of making them
US20080011390A1 (en) * 2006-07-11 2008-01-17 Clark Arthur E Galfenol steel
US20090025834A1 (en) * 2005-02-24 2009-01-29 University Of Virginia Patent Foundation Amorphous Steel Composites with Enhanced Strengths, Elastic Properties and Ductilities
US20100310901A1 (en) * 2007-09-18 2010-12-09 Japan Science And Technology Agency Metallic glass, magnetic recording medium using the same, and method of manufacturing the magnetic recording medium

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US5961745A (en) * 1996-03-25 1999-10-05 Alps Electric Co., Ltd. Fe Based soft magnetic glassy alloy
US5976274A (en) * 1997-01-23 1999-11-02 Akihisa Inoue Soft magnetic amorphous alloy and high hardness amorphous alloy and high hardness tool using the same
US6284061B1 (en) * 1997-01-23 2001-09-04 Akihisa Inoue Soft magnetic amorphous alloy and high hardness amorphous alloy and high hardness tool using the same
US6077367A (en) * 1997-02-19 2000-06-20 Alps Electric Co., Ltd. Method of production glassy alloy
US6086651A (en) * 1997-08-28 2000-07-11 Alp Electric Co., Ltd. Sinter and casting comprising Fe-based high-hardness glassy alloy
US6183889B1 (en) * 1997-08-28 2001-02-06 Alps Electric Co., Ltd. Magneto-impedance element, and magnetic head, thin film magnetic head, azimuth sensor and autocanceler using the same
US6227985B1 (en) 1997-08-28 2001-05-08 Alps Electric Co., Ltd. Sinter and casting comprising Fe-based high-hardness glassy alloy
US6287514B1 (en) 1997-08-28 2001-09-11 Alps Electric Co., Ltd. Sinter and casting comprising Fe-based high-hardness glassy alloy
US6296681B1 (en) * 1997-08-28 2001-10-02 Alps Electric Co., Ltd. Sinter and casting comprising Fe-based high-hardness glassy alloy
US6331348B1 (en) 1997-10-20 2001-12-18 Alps Electric Co., Ltd. Substrate having repaired metallic pattern and method and device for repairing metallic pattern on substrate
US6875952B2 (en) 1997-10-20 2005-04-05 Alps Electric Co., Ltd. Substrate having repaired metallic pattern and method and device for repairing metallic pattern on substrate
US6350323B1 (en) 1999-01-08 2002-02-26 Alps Electronic Co., Ltd. High permeability metal glassy alloy for high frequencies
US6594157B2 (en) 2000-03-21 2003-07-15 Alps Electric Co., Ltd. Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US20030201032A1 (en) * 2000-03-21 2003-10-30 Shoji Yoshida Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US20030205295A1 (en) * 2000-03-21 2003-11-06 Shoji Yoshida Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US6750723B2 (en) 2000-03-21 2004-06-15 Alps Electric Co., Ltd. Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US6897718B2 (en) 2000-03-21 2005-05-24 Alps Electric Co., Ltd. Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
US20030164209A1 (en) * 2002-02-11 2003-09-04 Poon S. Joseph Bulk-solidifying high manganese non-ferromagnetic amorphous steel alloys and related method of using and making the same
US7067020B2 (en) 2002-02-11 2006-06-27 University Of Virginia Patent Foundation Bulk-solidifying high manganese non-ferromagnetic amorphous steel alloys and related method of using and making the same
US7517415B2 (en) 2003-06-02 2009-04-14 University Of Virginia Patent Foundation Non-ferromagnetic amorphous steel alloys containing large-atom metals
US7763125B2 (en) 2003-06-02 2010-07-27 University Of Virginia Patent Foundation Non-ferromagnetic amorphous steel alloys containing large-atom metals
US20060130944A1 (en) * 2003-06-02 2006-06-22 Poon S J Non-ferromagnetic amorphous steel alloys containing large-atom metals
US20060213587A1 (en) * 2003-06-02 2006-09-28 Shiflet Gary J Non-ferromagnetic amorphous steel alloys containing large-atom metals
US7132019B2 (en) 2004-04-22 2006-11-07 Alps Electric Co., Ltd. Amorphous soft magnetic alloy powder, and dust core and wave absorber using the same
US20050236071A1 (en) * 2004-04-22 2005-10-27 Hisato Koshiba Amorphous soft magnetic alloy powder, and dust core and wave absorber using the same
US20050263216A1 (en) * 2004-05-28 2005-12-01 National Tsing Hua University Ternary and multi-nary iron-based bulk glassy alloys and nanocrystalline alloys
US20090025834A1 (en) * 2005-02-24 2009-01-29 University Of Virginia Patent Foundation Amorphous Steel Composites with Enhanced Strengths, Elastic Properties and Ductilities
US9051630B2 (en) 2005-02-24 2015-06-09 University Of Virginia Patent Foundation Amorphous steel composites with enhanced strengths, elastic properties and ductilities
US20090249920A1 (en) * 2005-11-16 2009-10-08 Zhichao Lu Fe-based amorphous magnetic powder, magnetic powder core with excellent high frequency properties and method of making them
US20070258842A1 (en) * 2005-11-16 2007-11-08 Zhichao Lu Fe-based amorphous magnetic powder, magnetic powder core with excellent high frequency properties and method of making them
US20080011390A1 (en) * 2006-07-11 2008-01-17 Clark Arthur E Galfenol steel
US20100310901A1 (en) * 2007-09-18 2010-12-09 Japan Science And Technology Agency Metallic glass, magnetic recording medium using the same, and method of manufacturing the magnetic recording medium
US8377580B2 (en) * 2007-09-18 2013-02-19 Japan Science And Technology Agency Metallic glass, magnetic recording medium using the same, and method of manufacturing the magnetic recording medium
US8968891B2 (en) 2007-09-18 2015-03-03 Japan Science And Technology Agency Metallic glass, magnetic recording medium using the same, and method of manufacturing the magnetic recording medium

Also Published As

Publication number Publication date Type
DE69610156T2 (en) 2001-04-12 grant
JP3904250B2 (en) 2007-04-11 grant
EP0747498A1 (en) 1996-12-11 application
DE69610156D1 (en) 2000-10-12 grant
JPH08333660A (en) 1996-12-17 application
EP0747498B1 (en) 2000-09-06 grant

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